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Metal vapor synthesis of (C5Me5)2Sm(THF)2 and (C5Me4Et)2Sm(THF)2 and their reactivity with organomercurial reagents. Synthesis and X-ray structural analysis of (C5Me5)2Sm(C6H5)(THF)
Evans, William J.,Bloom, Ira,Hunter, William E.,Atwood, Jerry L.
, p. 112 - 119 (1985)
The reaction of samarium metal vapor with hexane solutions of C5Me5H and C5Me4EtH at -110 to -125 °C followed by suitable workup gives (C5Me5)2Sm and (C5Me4Et)2Sm, respectively, as well as products which dissolve in THF to give (C5Me5)2Sm(THF)2 and (C5Me4Et)2Sm(THF)2, respectively. Evidence is found for hydride- and nitrogen-containing intermediates that decompose to the above compounds upon workup. (C5Me5)2Sm(THF)2 reacts with Hg(C6H5)2 to form (C5Me5)2Sm(C6H5)(THF) that has been characterized by X-ray crystallography. The phenyl complex crystallizes in space group P21/c with unit-cell dimensions a = 9.680 (5) A?, b = 17.291 (7) A?, c = 17.140 (7) A?, β = 103.78 (4)°, and Z = 4 for Dcalcd = 1.36 g cm-3. Least-squares refinement on the basis of 3308 observed reflections led to a final R value of 0.034. The two C5Me5 ring centroids, the phenyl carbon attached to Sm, and the THF oxygen describe a distorted tetrahedral structure around Sm in a structure typical of bent metallocene derivatives. Average Sm-C (ring) distances are 2.73 (1) and 2.745 (9) A?, the Sm-C(phenyl) distance is 2.511 (8) A?, and the Sm-O(THF) distance is 2.511 (4) A?.
